This invention relates to soil-resistant spin finish compositions, a method for applying the compositions to synthetic fibers, and final fiber constructions made from synthetic fibers treated with the soil-resistant spin finish compositions.
Lubrication and finishing of yarns and threads, such as cotton and silk, has been practiced since ancient times. Such yarns and threads, derived from natural-occurring plants and animals such as cotton plants and silkworms, often required lubrication or finishing by xe2x80x9coilingxe2x80x9d or xe2x80x9csizingxe2x80x9d to facilitate spinning and bundling. Lubricants used were typically natural hydrophobic oils, such as mineral oil or coconut oil. Sometimes, molten waxes such as beeswax were employed which, when cooled, formed a solid lubricating finish. Usually, the fibers were xe2x80x9csizedxe2x80x9d by applying a lubricant and/or adhesive material to yarn or warp threads in a weaving operation to impart cohesion and lubricity. Historically, sizes have been hard coatings, applied neat and at a higher fiber add-on than spin finishes, and were often based on starch, wax, and other oleophilic materials. For example, U.S. Pat. No. 1,681,745 discloses a beeswax-based size for artificial silk (rayon) which is applied molten and solidifies quickly before the thread is wound up, thus assuring bundle cohesion and lubrication in all subsequent operations.
While sizes were useful in facilitating the spinning and bundling of fibers, their presence in finished articles was found to be undesirable. In particular, the oleophilic nature of the sizes was found to adversely effect the soil resistance of the finished article. Sizes also frequently compromised the appearance and handle of the article Consequently, it became common practice to remove the size from a woven article after its manufacture by scouring the article in hot and/or detergent-containing water. In some instances, these sizes were also removed or reduced to acceptable levels as an inherent part of the dying process, as when the woven article is dyed through immersion in aqueous dye baths. However, this later methodology, in which the scouring and dying steps were effectively combined into a single process, also had its drawbacks. In particular, the presence of sizes in the dye bath frequently had adverse affects on the dying process, while also necessitating frequent replenishment of the dye solution.
After World War II, fibers were introduced which were made from synthetic polymers such as nylon, polyolefin, polyester and acrylic. These new high performance synthetic fibers required the use of special sizes called xe2x80x9cspin finishesxe2x80x9d during spinning and the subsequent fiber operations (e.g., bundling or sizing) required to produce the final woven article (e.g., fabric or carpet). The spin finish served several functions, including (1) reducing the friction developed as the synthetic fibers passed over metal and ceramic machinery surfaces, (2) imparting fiber-to-fiber lubricity, (3) minimizing electrical static charge buildup (a problem especially pronounced in the manufacture of woven articles from synthetic fibers), and, in some instances, (4) providing cohesion to the fiber. In addition, with proper use of additives, spin finish compositions could be made that were stable to high temperatures and pressures, had a controllable viscosity under application conditions, were non-corrosive, and were relatively safe to both the workers and the environment. (See Pushpa, B. et al., xe2x80x9cSpin Finishes,xe2x80x9d Colourage, Nov. 16-30, 1987 (17-26)). However, as with their sizing predecessors, the spin finishes had to be removed from the articles woven from the fibers, typically by scouring, to minimize soiling problems See, e g., U.S. Pat. No. 5,263,308 (Lee et al.), Col. 2, Lines 23-25.
The process of scouring is very undesirable in that it is a tedious process which adds to manufacturing costs, while also posing water pollution problems and health concerns. See, e.g., U.S. Pat. No. 5,263,308 (Lee et al.), Col. 2, Lines 20-24. Accordingly, some attempts have been made to avoid the need for scouring by treating unscoured carpets with agents that improve the soil resistance, handle, and other characteristics of the unscoured carpet to levels acceptable for the intended end use. Thus, U.S. Pat. No. 5,756,181 (Wang et al.) and U.S. Pat. No. 5,738,687 (Kamrath et al.) describe the treatment of unscoured carpet with certain polycarboxylate salts to achieve desirable soil resistance and repellency characteristics. Similarly, U.S. Ser. No. 08/595,592 (Wang et al.) describes the topical treatment of unscoured carpets with various inorganic agents such as silica to improve the soil resistance of the carpet. However, while these treatments are notable improvements in the art and work quite well in certain end uses, the requirement of a polycarboxylate salt and/or an inorganic additive is not desirable for all applications.
Other methods have been proposed in the art that are aimed at removing soil-attracting fiber finishes while avoiding the need for scouring and, in some cases, the need for additional treatment agents However, most of these methods have proven impractical in a commercial setting. For instance, Japanese Patent 2,572,503 describes a polyether oil spin finish that is sublimed or decomposed from spun-out yarn by heating the treated yarn to 180-220xc2x0 C. Unfortunately, the high temperatures required for this process have an adverse effect on the yarn, and the sublimation process itself is undesirable because of the energy and pollution problems attendant thereto. Accordingly, it remains the conventional practice in the art to remove spin finishes by scouring.
Most spin finishes currently known to the art are aqueous emulsions or dispersions, although some neat spin finishes are also known. The former are frequently preferred to neat spin finishes because the larger volume of finish applied per fiber weight results in lower application variability. Additionally, the water helps eliminate troublesome static charge, especially when formulated with other additives. (See Postman, W., xe2x80x9cSpin Finishes Explained,xe2x80x9d Textile Research Journal, July 1980 (444-453). Also, aqueous emulsions and dispersions frequently have lower viscosities, and therefore better frictional properties, than neat systems, and are easier to remove by scouring or during the dyeing process. See, e.g., R. J. Crossfield, xe2x80x9cApplying Spin Finishes for Optimum Downstream Fiber Qualityxe2x80x9d (Aug. 18, 1998), and R. J. Crossfield, xe2x80x9cLubricants for Synthetic Fibersxe2x80x9d (Jul. 24, 1998), both publications of Goulston Technologies, Inc.
The patent literature describes the use of a wide variety of aqueous emulsions or dispersions as components of various fiber treatments or finishes. These materials are typically removed by scouring with hot water and/or detergent, or by other methods (e.g., as an inherent part of immersion dying) to avoid the detrimental affect of the finish on the soiling properties of the final article of commerce.
U.S. Pat. No. 4,388,372 (Champaneria et al.) describes an improved process for making soil-resistant filaments of a synthetic linear polycarbonamide, preferably 6-nylon and 66-nylon, by applying a water-borne primary spin finish composition comprising a perfluoroalkyl ester, a modified epoxy resin and a non-ionic textile lubricant based on poly(ethylene glycol). Particularly preferred lubricants include n-butyl initiated random copolymers of ethylene/propylene oxide. At Col. 6, Lines 59-61 of the reference, it is noted that xe2x80x9cExcessive amounts of textile lubricants in the finish composition can interfere in the durability and effectiveness of the soil-resistant ingredients.xe2x80x9d Accordingly, much of the lubricant is removed at a later stage of processing when the filaments are subjected to a scouring or dyeing operation (Col. 6, lines 51-55), and application of a secondary fiber finish composition to the spun yarn is recommended at the point between the take up and windup rolls (Col. 12, lines 18-19).
U.S. Pat. No. 5,139,873 (Rebouillat) discloses aromatic polyamide fibers which are said to be highly processable and to have high modulus, improved surface frictional properties, scourability, deposition, fibrillation and antistatic properties. The fibers have a coating consisting of (a) 30-70% by weight of a long chain carboxylic acid ester of a long chain branched primary or secondary, saturated, monohydric alcohol, (b) 20 to 50% by weight of an emulsifying system consisting of certain nonionic surfactants, with the remainder being an antistatic agent, a corrosion inhibitor or other optional additives. The scourability of the coating is said to be very important as the residual finish level impacts the subsequent finishing in the case of fabrics (Col. 11, Lines 52-56).
U.S. Pat. No. 5,263,308 (Lee et al.) describes a method for ply-twisting nylon yarns (already spun) at high speeds by coating the nylon fibers with less than about 1% by weight of a finish containing an alkyl polyoxyethylene carboxylate ester lubricant composition of the general formula R1xe2x80x94Oxe2x80x94Xnxe2x80x94(CH2)mC(O)xe2x80x94Oxe2x80x94R2, where R1 is an alkyl chain from 12 to 22 carbon atoms, X is xe2x80x94C2H4Oxe2x80x94 or a mixture of xe2x80x94C2H4Oxe2x80x94 and xe2x80x94C3H6Oxe2x80x94, n is 3 to 7, m is 1 to 3, and R2 is an alkyl chain from 1 to 3 carbon atoms. The resulting ply-twisted yarn is especially suitable for use as pile in carpets. The reference notes that these lubricants are advantageous over other lubricants in that they may be applied at very low levels and afford ease of wash-off during dying or scouring operations, both of which lead to improved soiling repellency (see Col. 5, Lines 10-36).
On class of materials that has found applicability in the fiber finish art are polyoxyalkylenes. These materials have been used as minor components in various fiber finish formulations and, in some instances, have also been used as secondary spin finishes.
British Patent Specification 1,189,581 describes a process for treating dyed or undyed cellulose-esters or synthetic fibers or yarns, or mixtures thereof, to improve their lubrication against polished metal machine parts and to change the physical characteristics of the fibers or yarns so as to facilitate weaving. Compounds used to treat the fibers or yarns include compounds of the general formula R1C(O)Oxe2x80x94Yxe2x80x94R2, where R1 is a straight or branched chain hydrocarbon residue containing from 5 to 17 carbon atoms, R2 is a short chain hydrocarbon residue containing 1 or 2 carbon atoms, and Y is a polyglycol residue containing from 3 to 16 alkylene oxide groups with 2 or 3 carbon atoms in the alkylene chain. The ability to remove the compound by washing (i.e., scouring) is required for possible later dying operations.
U.S. Pat. No. 5,246,988 (Wincklhofer et al.) describes the use of lubricants, which are the reaction product of 1 mole of either a C5-C36 fatty acid or alcohol with 2 to 20 moles of ethylene oxide, as carriers for hindered amine anti-oxidants. These anti-oxidants/carriers are used to treat articles of high molecular weight thermoplastic films and fibers, thereby rendering the articles stable to heat and aging and allowing them to retain their breaking strength. Preferably, the lubricant comprises polyalkylene glycol (400) perlargonate, polyalkylene glycol (200) monolaurate and/or polyalkylene glycol (600) monoisostearate.
U.S. Pat. No. 3,770,861 (Hirano et al.) describes compositions of the formula R1xe2x80x94C(O)xe2x80x94Oxe2x80x94Axe2x80x94C(O)xe2x80x94R2, R1xe2x80x94Oxe2x80x94Axe2x80x94C(O)xe2x80x94R2 and R1xe2x80x94Oxe2x80x94Axe2x80x94H, wherein R1 and R2 are each alkyl, aralkyl or alkaryl groups of 2-26 carbon atoms, and wherein A can be (CH2CH2O)n, where n is an integer not less than 1. These compositions are used as melt-adhesion preventors for the super-drawing of melt-spinnable polyester fibers.
U.S. Pat. No. 5,399,616 (Kuhn et al.) describes lubricant-containing aqueous preparations obtained by polymerizing a monomer mixture of an ethylenically unsaturated carboxylic acid, a sulfonated aliphatic or aromatic monovinyl compound and an N-substituted vinyl amide in the presence of a polyol which has been esterified with a fatty acid of 8 to 26 carbon atoms. The preparation comprises 70-95% monomer mixture and 5-30% esterified polyol. The preparations are used as a low friction additive in dyeing and textile auxiliaries and, in particular, to prevent crease marks during textile wet processing. No mention is made of fiber lubricants or soil-resistant properties.
U.S. Pat. No. 5,491,004 (Mudge et al.) describes a method for applying a low soil finish to textile fibers as a secondary finish, i.e., a finish applied subsequent to fiber spinning. This method comprises applying to the spun fibers a low soil finish composition containing a dry, waxy solid component which can comprise the reaction product of a C8-C22 fatty acid ester with from 2 to 250 moles of ethylene oxide. Treated fibers and fabrics and carpets made therefrom are claimed to exhibit excellent soil-resistance. However, since this fatty acid ester composition is recommended when a cleanable, i.e., removable, low soil fiber finish is desired (Col. 3, Lines 22-27), the reference does not address the more difficult challenge of developing a low soiling primary finish.
Research Disclosures 16949 and 19520, xe2x80x9cNew Finishes,xe2x80x9d May 1978 and July 1980, disclose finishes useful for treating industrial fibers, such as polyamide and aramide fibers and yarns. These finishes can contain up to 40 parts (per hundred) of polyethylene glycol (400-600) monostearate and 15 parts of polyethylene glycol distearate and are apparently applied as secondary finishes.
U.S. Pat. No. 4,883,604 (Veitenhansl et al.) describes compositions and methods for smoothing textile fibers and sheet-form textiles made from the fibers. These compositions, which are described as solutions, emulsions, or aqueous dispersions, contain a combination of aliphatic polyether having C6-C24 alkyl radicals and containing 1 to 25 units of polymerized C2-C6 alkylene oxides and oxidized, high-density polyethylene. The concentration of aliphatic polyether in these compositions is from 5% to 30%, with the remainder of the composition being dispersants, softeners, other additives, and water. The compositions are used to improve stitching characteristics of the sheet-formed textiles, and no mention is made of improving soil-resistance or repellency.
Other references of note include U.S. Pat. No. 5,153,046 (Murphy), which describes an aqueous finish composition for imparting soil-resistant protection to textile fibers, e.g., nylon yarn. The composition is said to be stable to the high shear environment of a fiber finish application system. This composition is composed of 1-35% (weight) of nonionic fluorochemical textile anti-soilant, 65-95% of nonionic water-soluble or water-emulsifiable lubricant, and 0.05-15% each of quaternary ammonium or protonated amine surfactant and nonionic surfactant. Preferred lubricants are polyethylene glycol 600 monolaurate and methoxypolyethylene glycol 400 monopelargonate.
A new proprietary spin finish composition for use with nylon and polypropylene fibers has been marketed by the George A. Goulston Co. (Monroe, N.C.) under the trade designation NF-5338. Although this spin finish composition, which is believed to be primarily composed of alkylated polyethylene glycol having more than 13 ethylene oxide units (i.e., having a PEG molecular weight of at least 600), is described as xe2x80x9csoil resistantxe2x80x9d, it does not exhibit the level of soil-resistance required for many applications.
While the finishes described in the above noted references have certain advantageous features, most of these finishes are either secondary spin finishes, or are not spin finishes at all. Hence, these references do not address the more strenuous requirements of a primary spin finish. Moreover, these references do not disclose a method for providing a primary spin finish to fibers which avoids the need for scouring.
Accordingly, there still exists a need in the art for a spin finish composition which can be applied to a fiber at the earliest stages of spinning, which can remain on the fiber all the way through the final fiber construction (typically carpet), which will enhance, or at least not compromise, the soil-resistant and repellency performance of the final fiber construction, and which does not require the use of other agents (e.g., inorganic additives or polycarboxylate salts) to exhibit desirable soil resistance properties. These and other needs are met by the current invention, as hereinafter described.
In one aspect, the present invention relates to a soil-resistant spin finish composition and a method of using the same. The spin finish composition can be applied to a fiber at the earliest stages of spinning, can remain on the fiber through the entire manufacturing process, and can be left on the fiber in the final article of commerce. The spin finish composition provides excellent fiber lubrication during high-speed spin processing, yet is sufficiently soil resistant to negate the need for scouring the final fiber construction, even absent the presence of additional coatings or agents.
The spin finish composition of the present invention comprises at least about 35% by weight of spin finish solids comprising a derivatized polyether selected from the group consisting of Formula I and Formula II:
R1Axe2x80x94(R2O)nR2xe2x80x94Bxe2x80x94R3xe2x80x83xe2x80x83(Formula I)
G[(R4O)axe2x80x94R4xe2x80x94Dxe2x80x94R5]txe2x80x83xe2x80x83(Formula II)
wherein:
R1 is an alkyl group or alkaryl group containing at least 13 carbon atoms, and preferably is a saturated alkyl group containing between 17 to 21 carbon atoms, inclusive;
R2 is xe2x80x94C2H4xe2x80x94, xe2x80x94C3H6xe2x80x94 or xe2x80x94C4H8xe2x80x94 or, when adjacent to a xe2x80x94C(O)xe2x80x94 moiety of A or B, can be xe2x80x94CH2xe2x80x94;
R3 is hydrogen or is an alkyl group containing between 1 and 22 carbon atoms inclusive;
R4 is either xe2x80x94C2H4xe2x80x94, xe2x80x94C3H6xe2x80x94 or C4H8xe2x80x94 or, when adjacent to a xe2x80x94C(O)xe2x80x94 moiety of D, can be xe2x80x94CH2xe2x80x94;
R5 is an alkyl group containing at least 13 carbon atoms, and preferably is a saturated alkyl group containing between 16 and 21 carbon atoms, inclusive;
A is independently selected from the group consisting of xe2x80x94C(O)Oxe2x80x94, OC(O)xe2x80x94, xe2x80x94C(O)NHxe2x80x94, xe2x80x94NHC(O)xe2x80x94, xe2x80x94Oxe2x80x94, xe2x80x94NHC(O)Oxe2x80x94, xe2x80x94OC(O)NHxe2x80x94 and xe2x80x94NHC(O)NHxe2x80x94, and is preferably xe2x80x94C(O)Oxe2x80x94;
B is independently selected from the group consisting of xe2x80x94OC(O)xe2x80x94, C(O)Oxe2x80x94, xe2x80x94NHC(O)xe2x80x94, xe2x80x94C(O)NHxe2x80x94, xe2x80x94OC(O)NHxe2x80x94 and xe2x80x94NHC(O)NHxe2x80x94, and is preferably OC(O)xe2x80x94; and
n is between 1 and 20, and preferably between 4 and 10;
with the proviso that, when R3 is hydrogen, B is xe2x80x94Oxe2x80x94 (i.e., forming an alcohol group), and with the additional proviso that, when A is xe2x80x94C(O)Oxe2x80x94 and B is xe2x80x94OC(O)xe2x80x94, n is between 1 and 12;
G is the residue from a polyfunctional nucleophilic initiating species, such as from pentaerythritol, trimethylolpropane or glycerol;
D is selected from the group consisting of xe2x80x94C(O)Oxe2x80x94, xe2x80x94OC(O)xe2x80x94, xe2x80x94C(O)Nxe2x80x94, xe2x80x94NHC(O)xe2x80x94, xe2x80x94NHC(O)Oxe2x80x94, xe2x80x94OC(O)NHxe2x80x94 and xe2x80x94NHC(O)NHxe2x80x94, and is preferably xe2x80x94OC(O)xe2x80x94;
a is at least 1; and
b is either 3 or 4
and may comprise at least 73% by weight, based on the total weight of solids in the spin finish, of said polyether. The spin finish may also comprise less than about 10% by weight, based on the total weight of spin finish solids, of fluorochemical, and less than about 1% by weight, based on the total weight of spin finish solids, of an antistat. The antistat may be, for example, polyethylene glycol lauryl phosphoric acid. The spin finish may also comprise less than about 1% by weight, based on the total weight of spin finish solids, of an emulsifier, such as, for example, sodium dodecylbenzene sulfonate.
As used herein, the term xe2x80x9cprimary spin finishxe2x80x9d refers to a spin finish which is applied to synthetic fibers soon after they are extruded from the spinneret, cooled, and bundled, but prior to drawing.
Thermoplastic polymers useful for making synthetic fibers of this invention include fiber-forming poly(alpha)olefins, polyamides, polyesters and acrylics. Preferred thermoplastic polymers are poly (alpha)olefins, including the normally solid, homo-, co- and terpolymers of aliphatic mono-1-olefins (alpha olefins) as they are generally recognized in the art. Usually, the monomers employed in making such poly(alpha)olefins contain 2 to 10 carbon atoms per molecule, although higher molecular weight monomers sometimes are used as comonomers. Blends of the polymers and copolymers prepared mechanically or in situ may also be used. Examples of monomers that can be employed in the invention include ethylene, propylene, butene-1, pentene-1, 4-methyl-pentene-1, hexene-1, and octene-1, alone, or in admixture, or in sequential polymerization systems. Examples of preferred thermoplastic poly(alpha)olefin polymers include polyethylene, polypropylene, propylene/ethylene copolymers, polybutylene and blends thereof. Polypropylene is particularly preferred for use in the invention.
Processes for preparing the polymers useful in this invention are well known, and the invention is not limited to a polymer made with a particular catalyst or process.
In accordance with the present invention, a molten thermoplastic polymer fiber can be extruded through a spinneret to form a plurality of filaments (typically around 80 filaments), each filament typically having a delta-shaped cross section. The filaments are cooled, typically by passing through an air quenching apparatus maintained at or slightly below room temperature. The filaments are then bundled and directed across guides or kiss rolls, whereupon they are treated with a molten spin finish of this invention. After receiving the spin finish treatment, the filaments are generally stretched. Stretching may be accomplished over a number of godets or pull rolls that are at elevated temperatures (e.g., from 85-115xc2x0 C.) sufficient to soften the thermoplastic polymer. By rotating the rolls at different speeds, stretching of the filaments can be obtained. While stretching can be accomplished in one step, it may be desirable to stretch the filaments in two steps. Typically, the filaments will be stretched 3 to 4 times the extruded length (i.e., stretched at a ratio of from 3:1 to 4:1). Subsequent to stretching, and in order to obtain a carpet yarn, it is desirable to texture the yarn with pressured air at an elevated temperature (e.g., 135xc2x0 C.) or steam jet and to subject it to crimping or texturizing.
Spin finishes can be applied to fibers at different stages of the production process, depending upon what balance of performance properties are demanded from the fiber at that particular production stage. A primary spin finish is generally applied to the fibers soon after they are extruded from the spinneret, cooled, and bundled, but prior to drawing, texturizing or crimping the fiber. The primary spin finish reduces fiber-to-metal or fiber-to-ceramic friction while the fiber travels along the early stage production equipment.
Application of a secondary spin finish is often necessary during the later stage production (i.e., after stretching, crimping and texturizing of the fiber). Weaving often requires higher bundle cohesion than can be tolerated during spinning of staple fibers. The secondary spin finish imparts greater adhesion and friction to the yarn or rope made from the yarn.
While ideally the primary spin finish would have properties which eliminate the need for any secondary spin finish, this is not always possible. For example, during production, fiber-to-metal or fiber-to-ceramic friction should be low, but the final article (rope, for example) may benefit from higher friction. A primary spin finish must be optimized to allow the initial stages of yarn production to proceed in an efficient manner. If the succeeding stages have different requirements, a secondary finish will have to be applied. A secondary finish will also have to be applied if the primary spin finish is removed, or almost removed, during a processing step. For example, the majority of primary spin finish is removed during dyeing of yarn or cloth in aqueous dyeing baths. Examples of these considerations abound in the cited literature.
Derivatized polyethers suitable for use in the soil-resistant spin finish compositions of the present invention include those given by the formula CnH2n+1C(O)O(C2H4O)kCmH2mOC(O)CnH2n+1, wherein k is between 1 and 20, m is between about 1 and about 22, and n is at least 13 as well as the following compounds:
C17H35C(O)O(C2H4O)3.5C2H4OC(O)C17H35 
C17H35C(O)O(C2H4O)6C2H4OC(O)C17H35 
C17H35C(O)O(C2H4O)8C2H4OC(O)C17H35 
C17H35C(O)O(C2H4O)8C2H4OH
C17H35C(O)O(C2H4O)7C2H4OCH3 
C21H43C(O)O(C2H4O)8C2H4OC(O)C21H43 
C17H35C(O)O(C3H6O)2C3H6OCH3 
C17H35C(O)O(C3H6O)2C3H6OC4H9 
C17H35C(O)O(C3H6O)2C3H6OC(O)C17H35 
C15H31C(O)O(C2H4O)8C2H4OC(O)C15H31 
C13H27C(O)O(C2H4O)8C2H4OC(G)C13H27 
C21H43C(O)O(C2H4O)8C2H4OC(O)C21H43 
C18H37O(C2H4O)8C2H4OC(O)C17H35 
C8H17C6H4O(C2H4O)8C2H4OC(O)C17H35 
C18H37OC(O)CH2O(C2H4O)4CH2C(O)OC18H37 
C17H35C(O)NHC3H6O(C2H4O)11C3H6NHC(O)C17H35 
CH3O(C2H4O)12C3H6NHC(O)C17H35 
C17H35NHC(O)CH2O(C2H4O)4CH2C(O)NHC17H35 
C18H37NHC(O)O(C2H4O)7C2H4OCH3 
C18H37NHC(O)O(C3H6O)6C3H6OC(O)NHC18H37 
C17H35C(O)O(C2H4O)4CH2xe2x80x94Cxe2x80x94[CH2O(C2H4O)4C(O)C17H35]3 
CH3CH2Cxe2x80x94[CH2O(C2H4O)2C(O)C17H35]3 
These polyethers may be blended with sufficient carrier (water and/or solvent) to provide a fluid spin finish composition which can be applied to fibers using conventional spin finish application equipment, at levels within the range of about 0.2% SOF (weight per cent solids on fiber) to about 4% SOF, more preferably from about 0.5% SOF to about 2% SOF, and most preferably from about 0.75% SOF to about 1.4% SOF. Water is preferred as the major component of the carrier. Suitable solvents which can be used alone or in combination with water include acetates (e.g., ethyl acetate), alcohols (e.g., ethanol) and glycol ethers (e.g., propylene glycol monopropyl ether).
The following optional additives may also be incorporated into an aqueous dispersion containing the soil-resistant spin finish composition of the present invention (percentages are given as weight percent solids of the spin finish)
(a) a fluorochemical repellent (typically up to 20%),
(b) an antistat (typically up to 5%), and
(c) an emulsifier (typically up to 1%).
Examples of useful fluorochemical repellents include fluorochemical urethanes, ureas, biurets, isocyanurates, carbodiimides, allophanates, esters, guanidines, oxazolidinones, acrylate polymers, ethers, alcohols, epoxides, amides, amines (and salts thereof) and acids (and salts thereof). These fluorochemical repellents are generally oligomers or polymers containing rod-like pendant fluorochemical groups which orient in a comb-like structure at the air interface to provide water, oil and soil repellency. The pendant fluorochemical groups are generally of the structure CnF2n+1[QN(Rxe2x80x2)]a(CH2)bxe2x80x94, wherein n is an integer from 4 to 12, Q is either xe2x80x94C(O)xe2x80x94 or xe2x80x94SO2xe2x80x94, Rxe2x80x2 is H or an alkyl group having from 1 to four carbon atoms, a is either 1 (present) or 0 (absent), and b is an integer from 1 to 12. The fluorochemical repellent should be incorporated in the spin finish composition at a sufficient level to provide oil and/or water repellency to the finished fiber, i.e., providing at least about 0.01% SOF, and preferably at least about 0.02% SOF.
Examples of useful antistats and emulsifiers are described by W. Postman in xe2x80x9cSpin Finishes Explained,xe2x80x9d Textile Research Journal July 1980 (444-453).
Derivatized Polyethetsxe2x80x94Preparation, Sources
PEG400MS (polyethylene glycol 400 monostearate)xe2x80x94100 g (0.25 mol) of CARBOWAX(trademark) 400 diol (commercially available from Union Carbide Corp., Danbury, Conn.) was combined with 71 g (0.25 mol) of stearic acid in 400 g of toluene in a 3-necked flask equipped with stirrer, heating mantle, thermometer and condenser. The contents were heated, azeotroped dry using a Dean Stark trap, and were allowed to cool. Next, 1.0 g (0 5% by weight of solids) of p-toluene sulfonic acid was added, and the mixture was refluxed with stirring overnight with the continuous removal of water. Infrared analysis indicated no acid carbonyl remained. A solution of 0.5 g of NaHCO3 in deionized water was then added. The resulting two-phase system was stirred and the water and toluene were removed at 80xc2x0 C. using a ROTO-VAC(trademark) evaporator to produce the desired monoester, C17H35C(O)O(C2H4O)8C2H4OH. This monostearate and its constituent reactants are presented as the first entry in TABLE 1.
The following esterified polyethers, also listed in TABLE 1, were made using essentially the same procedure as described for polyethylene glycol 400 monostearate, except (1) the CARBOWAX(trademark) 400 glycol was replaced by CARBOWAX(trademark) glycols or CARBOWAX(trademark) monomethyl ether alcohols (MPEG) having polyethylene glycol (PEG) segments of varying molecular weights, or the CARBOWAX(trademark) 400 glycol was replaced by tripropylene glycol (TPG), its methyl ether alcohol (MTPG) or butyl ether alcohol (BuTPG) and/or (2) the stearic acid was replaced by another carboxylic acid such as behenic acid, palmitic acid or myristic acid at the desired mole ratio All raw materials used in TABLE 1 are commercially available from Aldrich/Sigma Chemical Co., Milwaukee, Wis.
TP-70TS (Trimethylolpropane Triethoxylate TP-70 tristearate)xe2x80x94To a 3-necked round-bottom flask equipped with stirrer, heating mantle and thermometer was added 50 g (0.1146 mol) of Trimethylolpropane Triethoxylate TP-70 (ave. Mn 430) (commercially available from Perstorp Polyols, Perstorp, Sweden), 97.9 g (0.344 mol) of stearic acid, 150 g of toluene and 1% by weight of total solids of CH3SO3H. This mixture was heated to reflux for 15 hours using a Dean-Stark apparatus. Next, 1% by weight of Ca(OH)2 was added to the mixture and the precipitate formed was filtered hot. The toluene was removed under vacuum using a ROTO-VAC(trademark) evaporator. The remaining solid showed no xe2x80x94OH peak by infrared analysis, indicating the reaction had progressed to completion to form the desired product, C2H5xe2x80x94C[CH2O(CH2CH2O)nC(O)C17H35]3.
PP-150TS (Pentaerythritol Tetraethoxylate PP-150 tetrastearate)xe2x80x94To a 3-necked round-bottom flask equipped with stirrer, heating mantle and thermometer was added 50 g (0.0625 mol) of Pentaerythritol Tetraethoxylate PP-150 (ave. Mn 800) (commercially available from Perstorp Polyols), 71.1 g (0.25 mol) of stearic acid, 150 g of toluene and 1% by weight of total solids of CH3SO3H. This mixture was heated to reflux for 15 hours using a Dean-Stark apparatus. Next, 1% by weight of Ca(OH)2 was added to the mixture and the precipitate formed was filtered hot. The toluene was removed under vacuum using a ROTO-VAC(trademark) evaporator. The remaining solid showed no xe2x80x94OH peak by infrared analysis, indicating the reaction had progressed to completion to give the desired product, Cxe2x80x94[CH2O(CH2CH2O)4]4C(O)C17H35.
ED-600DSA (JEFFAMINE(trademark) ED-600 distearamide)xe2x80x94To a 3-necked round-bottom flask equipped with stirrer, heating mantle and thermometer were added 100 g (0.1666 mol) of JEFFAMINE(trademark) ED-600 polyoxyethylene diamine (commercially available from Huntsman Chemical Co., Houston, Tex.), 47.4 g (0.3332 mol) of stearic acid, and 0.15 g (0.1 wt %) of IRGANOX(trademark) 1010 antioxidant (commercially available from Ciba-Geigy Corp., Greensboro, N.C.). The mixture was heated at 150xc2x0 C. under nitrogen for 2-3 hours, followed by heating at 180-200xc2x0 C. for an additional 7-8 hours. Infrared spectroscopy of this material showed an xe2x80x94NH peak at 3305 cmxe2x88x921 with the disappearance of xe2x80x94COOH and no primary amine peaks, confirming the formation of the distearamide, C17H35C(O)NHCH(CH3)CH2O(CH2CH2O)12CH2CH(CH3)NHC(O)C17H35.
ED-900DSA (JEFFAMINE(trademark) ED-600 distearamide)xe2x80x94This composition was prepared using essentially the same procedure as was described for preparing ED-600DSA, except that JEFFAMINE(trademark) ED-900 polyoxyethylene diamine (commercially available from Huntsman Chemical Co.) was substituted for JEFFAMINE(trademark) ED-600 polyoxyethylene diamine.
M-715MSA (JEFFAMINE(trademark) M-715 monostearamide)xe2x80x94This composition was prepared using essentially the same procedure as was described for preparing ED-600DSA, except that JEFFAMINE(trademark) M-715 methoxypolyoxyethylene monoamine (commercially available from Huntsman Chemical Co.) was substituted for JEFFAMINE(trademark) ED-600 polyoxyethylene diamine and the monostearamide, CH3O(CH2CH2O)15CH2CH(CH3)NHC(O)C17H35, was made instead of the distearamide.
PEG400DSU (polyethylene glycol 400 distearyl urethane)xe2x80x94To a 3-necked flask equipped with stirrer, heating mantle and thermometer were added 30.5 g (0.0762 mol) of CARBOWAX(trademark) 400 diol and 150 ml of toluene. The mixture was refluxed for 2-3 hours using a Dean-Stark apparatus. Some water ( less than 0.3 mL) was collected in Dean-Stark condenser and discarded. After cooling this mixture to 70xc2x0 C., 45.05 g (0.1524 mol) of octadecyl isocyanate (commercially available from Aldrich/Sigma Chemical Co.) and 1 drop of dibutyltin dilaurate catalyst were added, and the mixture was stirred at 70xc2x0 C. for 12 hours under nitrogen. Infrared spectral analysis of the reaction product showed an xe2x80x94NH peak at 3334 cmxe2x88x921 with the disappearance of xe2x80x94NCO peak, confirming the formation of the distearyl urethane, C18H37NHC(O)O(CH2CH2O)8C(O)NHC18H37. The toluene was evaporated under vacuum using a ROTO-VAC(trademark) evaporator.
PPG425DSU (polypropylene glycol 425 distearyl urethane)xe2x80x94To a 3-necked round-bottom flask equipped with stirrer, heating mantle and thermometer were added 50 g (0.0118 mol) of polypropylene glycol (number average mol. wt. of 525, commercially available from Sigma/Aldrich Chemical Co., Milwaukee, Wis.), 69.5 g (0.235 mol) of octadecyl isocyanate, 150 g of ethyl acetate and 2 drops of dibutyltin dilaurate catalyst. The mixture was heated at 75xc2x0 C. for 12 hours under nitrogen. IR analysis of this material showed a xe2x80x94NH peak at 3334 cmxe2x88x921 with the disappearance of xe2x80x94NCO peak confirming the formation of the distearyl urethane, C18H37NHC(O)O[CH2CH(CH3)O]9C(O)NHC18H37. The ethyl acetate was evaporated under vacuum using a ROTO-VAC(trademark) evaporator.
MPEG350MSU (methoxypolyethylene glycol 350 monostearyl urethane)xe2x80x94To a 2-necked, 1-L round bottom flask equipped with magnetic stirring bar, condenser and thermometer was added 100 g (0.286 mol) of MPEG350 and 84.4 g (0.286 mol) of octadecyl isocyanate (both commercially available from Aldrich/Sigma Chemical Co., Milwaukee, Wis.), 350 g of toluene and 2-3 drops of dibutyltin dilaurate. The mixture was heated to 55-60xc2x0 C. and was stirred gently for 8 hours. At this time, IR analysis showed total reaction of the isocyanate groups. The toluene was then stripped off and the urethane, CH3O(C2H4O)8C(O)N(H)C18H37, was isolated.
MPEG750MSU (methoxypolyethylene glycol 750 monostearyl urethane)xe2x80x94This composition was prepared using essentially the same procedure as was described for preparing MPEG350MSU, except that MPEG 750 methoxypolyoxyethylene alcohol was substituted for NPEG 350 methoxypolyoxyethylene alcohol.
MPEG2000MSU (methoxypolyethylene glycol 2000 monostearyl urethane)xe2x80x94This composition was prepared using essentially the same procedure as was described for preparing MPEG350MSU, except that MPEG 2000 methoxypolyoxyethylene alcohol was substituted for MPEG 350 methoxypolyoxyethylene alcohol.
NF-5338 Spin Finish Compositionxe2x80x94NF-5338 is a low-soiling spin finish formulation, commercially available from George A. Goulston Co., Monroe, N.C., believed to be primarily composed alkylated polyethylene glycol having more than 13 ethylene oxide units (i.e., having a PEG molecular weight of at least 600).
L-1D Carpetxe2x80x94carpet made from polypropylene fiber having coated thereon approximately 0.74% SOF of spin finish having the following composition (w/w): 10% PEG400DS, 1.4% MeFOSE600UU, 0.1% ETHFAC(trademark) 142W antistat (available from Ethox Chemicals, Greenville, S.C.) and the remainder being ethyl acetate.
SSC 6-789Axe2x80x94a commercial spin finish (available from SSC Industries, East Point, Ga.), believed to be a monoester of a 7-unit polyethylene oxide and lauric acid.
Fluorochemical Repellent Additivesxe2x80x94Preparation, Sources
FX-1373Mxe2x80x943M Brand FX-1373M Commercial Carpet Protector, commercially available from 3M Company, St. Paul, Minn.
FX-1860xe2x80x94SCOTCHGARD(trademark) FX-1860 Fabric Protector, commercially available from 3M Company
FC-365xe2x80x943M Brand FC-365 Carpet Protector, commercially available from 3M Company
FC-248xe2x80x94SCOTCHGARD(trademark) FC-248 Stain Release, commercially available from 3M Company
EtFOSE600Uxe2x80x94a fluorochemical polyoxyethylene urethane synthesized and emulsified according to the following process. Into a 3-necked flask equipped with an overhead stirrer, thermometer and reflux condenser with nitrogen inlet were placed 114 g (0.2 mole) of DESMODUR(trademark) N-100 triisocyanate (commercially available from Miles Corp., Pittsburgh, Pa.), 205 g (0.37 mol) of EtFOSE alcohol (C8F17SO2N(C2H5)C2H4OH, commercially available from 3M Company as FLUORAD(trademark) FC-10 fluorochemical alcohol), 200 g of methyl isobutyl ketone (MIBK) and 5 drops of dibutyltin dilaurate catalyst. The resulting mixture was heated to 80xc2x0 C. and was allowed to react overnight to complete the reaction. Then 75.6 g (0.126 mol) of CARBOWAX(trademark) 600 glycol (commercially available from Union Carbide Corp.) was added, the temperature was maintained at 80xc2x0 C., and the reaction was allowed to proceed until no free isocyanate was detectable by infrared spectroscopy, indicating that all isocyanate groups had been converted to urethane groups. Next, 166 g of the resulting polymer solution was mixed with 104 g of MIBK, and this mixture was emulsified in 400 g of deionized water containing 4% (w/w) of SIPONATE(trademark) DS-10 (sodium dodecylbenzene sulfonate, commercially available from Rhone-Poulenc, North America Chem., Surfactants and Specialties, Cranberry, N.J.) using a Branson SONIFIER(trademark) 450 ultrasonic horn (commercially available from VWR Scientific, West Chester, Pa.). The MIBK was removed under reduced pressure to yield an aqueous polymer dispersion containing approximately 25% fluorochemical solids
EtFOSE1450Uxe2x80x94a fluorochemical polyoxyethylene urethane, synthesized and emulsified using the same procedure as described for the preparation of EtFOSE600U, except that an equimolar quantity of CARBOWAX(trademark) 1450 glycol (commercially available from Union Carbide Corp.) was substituted for the CARPBOWAX(trademark) 600 glycol.
EtFOSE600UUxe2x80x94a fluorochemical polyoxyethylene urethane urea, synthesized using the following process. Into a 3-necked flask equipped with an overhead stirrer, thermometer and reflux condenser with nitrogen inlet were placed 114 g (0.2 mole) of DESMODUR(trademark) N-100 triisocyanate (commercially available from Miles Corp., Pittsburgh, Pa.), 183 g (0.33 mol) of C8F17SO2N(C2H5)C2H4OH (commercially available from 3M Company as FLUORAD(trademark) FC-10 fluorochemical alcohol), 200 g of methyl isobutyl ketone (MIBK) and 5 drops of dibutyltin dilaurate catalyst. The resulting mixture was heated to 80xc2x0 C. for 6 hours to complete the urethane reaction. Next, 1.35 g (0.075 mol) of deionized water was added, and the reaction mixture was allowed to react overnight at 80xc2x0 C. to complete the urea reaction. Finally, 45 g (0.075 mol) of CARBOWAX(trademark) 600 glycol (commercially available from Union Carbide Corp.) was added, the temperature was maintained at 80xc2x0 C., and the reaction was allowed to proceed until no free isocyanate was detectable by infrared spectroscopy, indicating that all isocyanate groups had been converted to urethane groups. A 25% solids (wt) emulsion was prepared using the same procedure earlier described for preparing the EtFOSE600 emulsion.
EtFOSE1450UUxe2x80x94a fluorochemical polyoxyethylene urethane, synthesized and emulsified using the same procedure as described for the preparation of EtFOSE600UU, except that an equimolar quantity of CARBOWAX(trademark) 1450 glycol was substituted for the CARBOWAX(trademark) 600 glycol.
MeFOSE600UUxe2x80x94a fluorochemical polyoxyethylene urethane, synthesized and emulsified using the same procedure as described for the preparation of EtFOSE600UU, except that an equimolar quantity of MeFOSE alcohol (C8F17SO2N(CH3)C2H4OH, available from 3M Company) was substituted for the MeFOSE alcohol.
MeFOSE1450UUxe2x80x94a fluorochemical polyoxyethylene urethane, synthesized and emulsified using the same procedure as described for the preparation of MeFOSE600UU, except that an equimolar quantity of CARBOWAX(trademark) 1450 glycol was substituted for the CARBOWAX(trademark) 600 glycol.
PEG400DS/MeFOSE1450UU Emulsionxe2x80x94prepared as follows.
First, a PEG400DS emulsion was prepared as follows. 200 g of PEG400DS was heated in an oven to 70xc2x0 C. to a molten state. In a separate bottle, 10 g of RHODACAL(trademark) DS-10 (available from Rhone Poulenc, Cranbury, N.J.) was dissolved in 1190 g of deionized water, and the resulting aqueous solution was heated to 70xc2x0 C. The molten PEG400DS was placed in a stainless steel beaker, stirred vigorously, and the aqueous solution was added. With continued stirring, a sufficient amount of 20% (w/w) aqueous NaOH was added to bring the pH up to around 6.0. The resulting mixture was then hydrogenized for 20 minutes using a BRANSON(trademark) Sonifier Ultrasonic Horn (available from VWR Scientific). The translucent emulsion produced was transferred to a polyethylene bottle, which was capped and rolled on a jar mill until cooled to around room temperature. The resulting PEG400DS emulsion was 15.2% (w/w) solids.
Next, MeFOSE1450UU was prepared as described in the synthesis of Fluorochemical Treatment E in U.S. Pat. No 5,672,651, except that the weight ratio used of MeFOSE fluorochemical alcohol to CARBOWAX(trademark) 1450 glycol to DESMODUR(trademark) N-100 isocyanate was 39.0:38.3:22.7 and ethyl acetate was used as the solvent rather than methyl isobutyl ketone. The resulting 30% (w/w) fluorochemical polyoxyethylene urethane urea solution in ethyl acetate was heated to 70xc2x0 C. Meanwhile, an aqueous solution consisting of 14.9 g RHODACAL(trademark) DS-10 in 550 g of deionized water was also pre-heated to 70xc2x0 C. The ethyl acetate solution was placed in a stainless steel beaker, stirred vigorously, and to it was added the aqueous solution. Using a 20% (w/w) aqueous NaOH solution, the pH of the resulting mixture was adjusted to 6 and the mixture was homogenized for 10 minutes using a BRANSON(trademark) Sonifier Ultrasonic Horn. The emulsion that formed was then placed in a 2 L round bottom flask and was vacuum stripped at 60xc2x0 C., resulting in a 17.7% (w/w) solids emulsion of MeFOSE1450UU.
To make the PEG400DS/MeFOSE1450UU emulsion, the above-described PEG400DS and MeFOSE1450UU emulsions were mixed at a 7.7:1 (v/v) ratio and the mixture was diluted with deionized water to give an emulsion containing 10% (w/w) PEG400DS and 1.5% (w/w) MeFOSE1450UU.
P250Telomerxe2x80x94a fluorochemical polyoxyethylene diester, prepared as follows. To a 3-necked round bottom flask equipped with stirrer, heating mantle and thermometer was added 25 g (0.1 mol) of polyethylene glycol bis-carboxymethyl methyl ether (ave. mol. wt. of 250, available from Sigma Aldrich, Milwaukee, Wis.), 102.8 g (0.2 mol) of Zonyl(trademark) BA-N alcohol (available from E. I. duPont de Nemours, Wilmington, Del.), 150 g of toluene and 1% by weight on solids of p-toluenesulfonic acid. The resulting mixture was heated to reflux for 15 hours using a Dean Stark apparatus. Next, 1% by weight on solids of Ca(OH)2 was added to the mixture and the precipitate formed was removed by filtration when still hot. Toluene was removed from the filtrate using a ROTO-VAC(trademark) evaporator. The remaining solid showed no xe2x80x94OH peak by infrared analysis, indicating the reaction had progressed to completion to form the desired product, F(CF2)nCH2CH2OC(O)CH2O(CH2CH2O)mCH2C(O)OCH2CH2(CF2)nF.
P250MeFOSExe2x80x94a fluorochemical polyoxyethylene diester, prepared using essentially the same procedure as was described for preparing P250Telomer except that C8F17SO2N(CH3)CH2CH2OH (MeFOSE alcohol) was substituted for Zonyl(trademark) BA-N alcohol.
FOSE linoleatexe2x80x94To a 3-necked round-bottom flask equipped with stirrer, heating mantle and thermometer was added 200 g (0.359 mol) of MeFOSE alcohol, 100 g (0.359 mol) of linoleic acid (available from Eastman Fine Chemicals, Rochester, N.Y.), 150 g of toluene and 1% by weight on solids of p-toluenesulfonic acid. The resulting mixture was heated to reflux for 15 hours using a Dean Stark apparatus. Next, 1% by weight on solids of Ca(OH)2 was added to the mixture and the precipitate formed was removed by filtration when still hot. Toluene was removed from the filtrate using a ROTO-VAC(trademark) evaporator. The remaining solid showed no xe2x80x94OH peak by infrared analysis, indicating the reaction had progressed to completion to form the desired product, C8F17SO2N(CH3)CH2CH2OC(O)(CH2)7CHxe2x95x90CHCH2CHxe2x95x90CH(CH2)4CH3.
FC adipatexe2x80x94a fluorochemical ester prepared as described in U.S. Pat. No. 4,264,484, Example 8, Formula XVII.
FC oxazolidinonexe2x80x94a fluorochemical oxazolidinone prepared by using essentially the same procedure as described in Scheme I of U.S. Pat. No. 5,025,052 (Crater et al.), reacting C8F17SO2N(CH3)CH(OH)CH2Cl with stearyl isocyanate at a 1:1 molar ratio followed by ring closure.
Test Methods
Fiber Spinning Procedurexe2x80x94Polypropylene resin having a melt-flow index of approximately 17 was melt-spun in the conventional manner through a spinneret at a rate of 91 g/min to provide 80 filaments with a delta-shaped cross-section. The molten filaments were then passed across an air quenching apparatus maintained at 60xc2x0 F. (15xc2x0 C.) whereupon solidification of the filaments occurred. The solid filaments were collected into a fibers which were directed across a slotted ceramic guide, where primary spin finish was applied by pump at a level of 0.75% solids on fiber (SOF). From the spin finish ceramic guide, the treated fiber traveled over a turnabout to the first godet. The fiber was wrapped 6 times around the first godet, said godet being heated to 85xc2x0 C. From the first godet, the fiber traveled to the second godet, where it was wrapped 6 times. The second godet was maintained at 115xc2x0 C. and its speed was adjusted to three times that of the first godet, thus drawing the fiber at a ratio of 3:1. From the second godet, the fiber traveled to a conventional hot air texturizer set at 135xc2x0 C. and 7 bar (700,000 Pa) pressure to form a yarn. The yarn then traveled to a third godet set at room temperature (i.e., about 25xc2x0 C.), where it was wrapped 6 times, and finally to a conventional winder. Fiber denier of the drawn and texturized fiber was maintained at approximately 1450 denier by adjustment of polymer output at the spinneret.
Coefficient of Friction Measurementxe2x80x94When measurement of coefficient of friction was desired, the yarn from the texturizer was wound 6 times around a fourth godet, across the tension transducer, across the friction pin, across the second tension transducer, 6 times around another godet and onto the winder.
At a given line speed, the apparent coefficient of friction (COF) between the fiber and the metal friction pin can be calculated using the following xe2x80x9ccapstanxe2x80x9d equation:
COF=ln(T1/T0)/q
where T1 is the tension on the fiber just before the metal friction pin, T0 is the tension on the fiber just after the metal friction pin, and q is the angle of contact in radians between the fiber and the metal friction pin. For all examples, T0 was standardized at 200 g and q was standardized at 3.002 radians (corresponding to the 25.4 mm diameter pin used). For all examples, the line speed was maintained at about 270 m/min.
The tension measurements were made using two Rothschild Permatens(trademark) measuring heads obtained from Lawson-Hemphill, Inc., Central Falls, R.I. Using a realtime data aquisition computer, the tension readings were recorded for each run at one second intervals over a 40-second time period.
A COF value of 0.30 or less is considered desirable, although COF values above 0.30 may be acceptable.
Determining Percent Lubricant on Fiberxe2x80x94The % SOF of spin finish composition actually coated onto the fiber was determined in accordance with the following test procedure.
An 8 g sample of spin finish-coated fiber is placed in an 8 oz (225 mL) glass jar along with 80 g of solvent (typically ethyl acetate or methanol). The glass jar is capped and placed on a roller mill for 10 minutes. Next, 50 g of the solvent containing the stripped lubricant is removed and is poured into a tared aluminum pan which is placed in a 250xc2x0 F. (121xc2x0 C.) vented oven for 20 minutes to evaporate the solvent. The pan is then reweighed to determine the amount of lubricant present, using the following calculations:
% SOF=(grams of finish extracted)/(5 grams)xc3x97100
Carpet Tufting Procedurexe2x80x94Samples of texturized fiber (i.e., yarn) were tufted into a level-loop style carpet at {fraction (5/32)} guage, 12 stitches per inch (5 stitches per centimeter) and 0.25 inch (0.64 cm) pile height.
Non-scoured (NS) control carpet was prepared from woven fiber treated with SSC 6-789A spin finish at approximately 0.75% SOF.
Scoured (S) control carpet was prepared from the non-scoured control carpet by continuously rotating the carpet through a Beck style hot water bath to remove the commercial spin finish, followed by spin extraction and drying.
xe2x80x9cWalk-Onxe2x80x9d Soiling Testxe2x80x94The relative soiling potential of carpet tufted from texturized fiber was determined by challenging both treated and untreated (control) carpet samples under defined xe2x80x9cwalk-onxe2x80x9d soiling test conditions and comparing their relative soiling levels. The test is conducted by mounting treated and untreated carpet squares on particle board, placing the samples on the floor of one of two chosen commercial locations, and allowing the samples to be soiled by normal foot traffic. The amount of foot traffic in each of these areas is monitored, and the position of each sample within a given location is changed daily using a pattern designed to minimize the effects of position and orientation upon soiling.
Following a specific soil challenge period, measured in number of cycles where one cycles equals approximately 10,000 foot-traffics, the treated samples are removed and the amount of soil present on a given sample is determined using calorimetric measurements. This method of measurement assumes that the amount of soil on a given sample is directly proportional to the difference in color between the unsoiled sample and the corresponding sample after soiling. The three CIE L*a*b* color coordinates of the unsoiled and subsequently soiled samples are measured using a Minolta 310 Chroma Meter with a D65 illumination source. The color difference value, xcex94E, is calculated using the equation shown below:
xcex94E=[(xcex94L*)2+(xcex94a*)2+(xcex94b*)2]xc2xd
where:
xcex94L*=L*soiledxe2x88x92L*unsoiled
xcex94a*=a*soiledxe2x88x92a*unsoiled
xcex94b*=b*soiledxe2x88x92b*unsoiled
xcex94E values calculated from these calorimetric measurements (usually an average of six replicates) are qualitatively in agreement with values from older, visual evaluations, such as the soiling evaluation suggested by the AATCC. These xcex94E values have the additional advantages of higher precision, being unaffected by evaluation environment or subjective operator differences. Generally, the number of cycles is chosen so that the xcex94E value for the soiled scoured carpet is around 3-4. A xcex94E value for unscoured carpet of no greater than 6 is considered desirable.
A xcex94xcex94E value can be readily calculated by subtracting the xcex94E value of soiled scoured carpet from the xcex94E value of soiled, spin finish-treated carpet. The xcex94xcex94E value is especially useful as it represents a direct comparison of soiling between spin finish-treated carpet and scoured carpet. Though xcex94xcex94E values can vary significantly depending upon carpet color and soiling conditions (e.g., winter vs. summer), a xcex94xcex94E value of no greater than about 3 is considered desirable.
Water Repellency Testxe2x80x94Carpet tufted from texturized fiber was evaluated for water repellency using 3M Water Repellency Test V for Floor coverings (February 1994), available from 3M Company. In this test, a carpet sample is challenged to penetrations by blends of deionized water and isopropyl alcohol (IPA). Each blend is assigned a rating number as shown below:
In running the Water Repellency Test, a treated carpet sample is placed on a flat, horizontal surface and the carpet pile is hand-brushed in the direction giving the greatest lay to the yarn. Five small drops of water or a water/IPA mixture are gently placed at points at least two inches apart on the carpet sample. If, after observing for ten seconds at a 45xc2x0 angle, four of the five drops are visible as a sphere or a hemisphere, the carpet is deemed to pass the test. The reported water repellency rating corresponds to the highest numbered water or water/IPA mixture for which the treated carpet sample passes the described test.
A water repellency value of at least 0, preferably at least 2 or higher, is considered desirable.
Oil Repellency Testxe2x80x94Carpet tufted from texturized fibers was evaluated for oil repellency using 3M Oil Repellency Test III (February 1994), available from 3M Company, St. Paul, Minn. In this test, a treated carpet sample is challenged to penetration by oil or oil mixtures of varying surface tensions. Oils and oil mixtures are given a rating corresponding to the following:
The Oil Repellency Test is run in the same manner as is the Water Repellency Test, with the reported oil repellency rating corresponding to the highest oil or oil mixture for which the treated carpet sample passes the test.
An oil repellency value of at least 1.5, preferably at least 2 or higher, is considered desirable.